原料药及药物制剂中美洛昔康的测定。

Determination of meloxicam in bulk and pharmaceutical formulations.

作者信息

Zawilla N H, Abdul-Azim Mohammad M, El kousy N M, El-Moghazy Aly S M

机构信息

National Organisation of Drug Control and Research, Cairo, Egypt.

出版信息

J Pharm Biomed Anal. 2003 Aug 21;32(6):1135-44. doi: 10.1016/s0731-7085(03)00232-2.

DOI:10.1016/s0731-7085(03)00232-2

PMID:12907256

Abstract

Three sensitive and reproducible methods for quantitative determination of meloxicam (mel) in pure form and in pharmaceutical formulations are presented. The first method is high performance liquid chromatography by which the drug is determined in the presence of its degradation products over concentration range 100-500 microg x ml(-1) with mean percentage accuracy 100.13+/-0.53. The second method is based on measuring the absorbance of the formed neutral complex between basic methylene blue and mel in phosphate buffer (pH 8) at lambda=653.5 nm over concentration range 1-5 microg x ml(-1) with mean percentage accuracy 99.12+/-1.18. The third method is based on reaction between 2,3-dichloro-5,6-dicyano-p-benzoquinone resulting in the formation of an intense orange red coloured product after heating in a boiling water bath for 5 min. The coloured product exhibits an absorption maximum at 455 nm, over concentration range 40-160 microg x ml(-1) with mean percentage accuracy 100.53+/-1.04.

摘要

本文介绍了三种灵敏且可重现的方法，用于定量测定纯品及药物制剂中的美洛昔康（mel）。第一种方法是高效液相色谱法，可在药物存在降解产物的情况下，于100 - 500 μg x ml⁻¹浓度范围内测定药物，平均百分准确度为100.13 ± 0.53。第二种方法基于在磷酸盐缓冲液（pH 8）中，在λ = 653.5 nm处测量碱性亚甲蓝与mel形成的中性络合物的吸光度，浓度范围为1 - 5 μg x ml⁻¹，平均百分准确度为99.12 ± 1.18。第三种方法基于2,3 - 二氯 - 5,6 - 二氰基对苯醌之间的反应，在沸水浴中加热5分钟后形成强烈的橙红色产物。该有色产物在455 nm处有最大吸收，浓度范围为40 - 160 μg x ml⁻¹，平均百分准确度为100.53 ± 1.04。